[go: up one dir, main page]
More Web Proxy on the site http://driver.im/

CN112707848A - Preparation method of guanidine hydrochloride - Google Patents

Preparation method of guanidine hydrochloride Download PDF

Info

Publication number
CN112707848A
CN112707848A CN201911021935.7A CN201911021935A CN112707848A CN 112707848 A CN112707848 A CN 112707848A CN 201911021935 A CN201911021935 A CN 201911021935A CN 112707848 A CN112707848 A CN 112707848A
Authority
CN
China
Prior art keywords
guanidine hydrochloride
reaction
preparation
dissolving
weight
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201911021935.7A
Other languages
Chinese (zh)
Inventor
方建文
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN201911021935.7A priority Critical patent/CN112707848A/en
Publication of CN112707848A publication Critical patent/CN112707848A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C277/00Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups
    • C07C277/02Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups of guanidine from cyanamide, calcium cyanamide or dicyandiamides
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C277/00Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups
    • C07C277/06Purification or separation of guanidine

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to a preparation method of a chemical product, in particular to a preparation method of guanidine hydrochloride, which comprises the following steps: a. melting, b, dissolving, c, filtering, d, dehydrating, e, crystallizing and obtaining the finished guanidine hydrochloride product with the yield higher than 95%. The reaction process is simple, the steps of adding raw materials, heating a reaction kettle and subsequent purification are not repeated, the energy consumption is reduced, the reaction time is shortened, byproducts are greatly reduced, and the yield is improved.

Description

Preparation method of guanidine hydrochloride
Technical Field
The invention relates to a preparation method of a chemical product, in particular to a preparation method of guanidine hydrochloride.
Background
In the existing production process of guanidine hydrochloride, dicyandiamide and ammonium salt (ammonium chloride) are generally used as raw materials, and are subjected to melt reaction at 170-230 ℃ to obtain a guanidine hydrochloride crude product, and the guanidine hydrochloride crude product is refined to obtain a finished product. In the refining process, raw materials need to be added repeatedly, the reaction kettle needs to be heated, and subsequent purification steps need to be carried out, so that the reaction energy consumption and the reaction time are greatly increased, and meanwhile, a large number of byproducts are generated and the yield is low.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: in order to overcome the defects in the prior art, an improved preparation method of guanidine hydrochloride is provided.
The technical scheme adopted by the invention is as follows: a preparation method of guanidine hydrochloride comprises the following steps:
a. melting: adding raw materials of dicyandiamide and ammonium chloride into a reaction kettle according to the weight ratio of 1: 1.27, adding a catalyst of zinc chloride, heating to 165 ℃, preserving heat for 3 hours, and carrying out a melting reaction to obtain a guanidine hydrochloride crude product;
b. dissolving: at normal temperature, dissolving the guanidine hydrochloride crude product in water according to the ratio of 1: 1;
c. and (3) filtering: removing raw materials, catalysts and reaction byproducts by a filtering method;
d. and (3) dehydrating: dehydrating the filtered mother liquor;
e. and (3) crystallization: cooling the supersaturated solution, concentrating and crystallizing to obtain a guanidine hydrochloride finished product;
wherein the input weight of the catalyst zinc chloride is 0.5 percent of the weight of the raw material dicyandiamide, and the weight percentage content of the guanidine hydrochloride in the finished product of the guanidine hydrochloride is more than 95 percent.
In the melting step, after heating to 165 ℃, the heating is stopped, the reaction is carried out for 3 hours, and the temperature is increased from 165 ℃ to 185 ℃. The melting reaction temperature is up to 185 ℃, and side reaction is difficult to occur at the temperature, so that byproducts are greatly reduced, and the yield is improved.
In the dissolving step, alkali is added into the solution so as to treat the residual ammonium salt in the reaction.
Compared with the prior art, the invention has the following advantages: the reaction process is simple, the steps of adding raw materials, heating a reaction kettle and subsequent purification are not repeated, the energy consumption is reduced, the reaction time is reduced, the reaction temperature is up to 185 ℃, byproducts are greatly reduced, and the yield is improved.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the embodiments of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
A preparation method of guanidine hydrochloride comprises the following steps:
a. melting: adding raw materials of dicyandiamide and ammonium chloride into a reaction kettle according to the weight ratio of 1: 1.27, adding a catalyst of zinc chloride, heating to 165 ℃, preserving heat for 3 hours, and carrying out a melting reaction to obtain a guanidine hydrochloride crude product;
b. dissolving: at normal temperature, dissolving the guanidine hydrochloride crude product in water according to the ratio of 1: 1;
c. and (3) filtering: removing raw materials, catalysts and reaction byproducts by a filtering method;
d. and (3) dehydrating: dehydrating the filtered mother liquor;
e. and (3) crystallization: cooling the supersaturated solution, concentrating and crystallizing to obtain a guanidine hydrochloride finished product;
wherein the input weight of the catalyst zinc chloride is 0.5 percent of the weight of the raw material dicyandiamide, and the weight percentage content of the guanidine hydrochloride in the finished product of the guanidine hydrochloride is more than 95 percent.
In the melting step, heating was stopped after heating to 165 ℃ and the reaction was stopped for 3 hours, and the temperature was raised from 165 ℃ to 185 ℃.
In the dissolving step, an alkali is added to the solution.

Claims (2)

1. The preparation method of guanidine hydrochloride is characterized by comprising the following steps:
a. melting: adding raw materials of dicyandiamide and ammonium chloride into a reaction kettle according to the weight ratio of 1: 1.27, adding a catalyst of zinc chloride, heating to 165 ℃, preserving heat for 3 hours, and carrying out a melting reaction to obtain a guanidine hydrochloride crude product;
b. dissolving: at normal temperature, dissolving the guanidine hydrochloride crude product in water according to the ratio of 1: 1;
c. and (3) filtering: removing raw materials, catalysts and reaction byproducts by a filtering method;
d. and (3) dehydrating: dehydrating the filtered mother liquor;
e. and (3) crystallization: cooling the supersaturated solution, concentrating and crystallizing to obtain a guanidine hydrochloride finished product;
wherein the input weight of the catalyst zinc chloride is 0.5 percent of the weight of the raw material dicyandiamide, and the weight percentage content of the guanidine hydrochloride in the finished product of the guanidine hydrochloride is more than 95 percent.
2. The method of preparing guanidine hydrochloride according to claim 1, wherein: in the dissolving step, alkali is added into the solution.
CN201911021935.7A 2019-10-25 2019-10-25 Preparation method of guanidine hydrochloride Pending CN112707848A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911021935.7A CN112707848A (en) 2019-10-25 2019-10-25 Preparation method of guanidine hydrochloride

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911021935.7A CN112707848A (en) 2019-10-25 2019-10-25 Preparation method of guanidine hydrochloride

Publications (1)

Publication Number Publication Date
CN112707848A true CN112707848A (en) 2021-04-27

Family

ID=75540546

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201911021935.7A Pending CN112707848A (en) 2019-10-25 2019-10-25 Preparation method of guanidine hydrochloride

Country Status (1)

Country Link
CN (1) CN112707848A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113754567A (en) * 2021-10-13 2021-12-07 宁夏蓝白黑循环科技有限公司 Novel preparation process of refined guanidine carbonate
CN115286538A (en) * 2022-07-12 2022-11-04 烟台三鼎化工有限公司 Antibacterial guanidine hydrochloride efficient crystallization drying process

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1385419A (en) * 2002-06-14 2002-12-18 方建文 Process for preparing guanidine hydrochloride
CN102079725A (en) * 2011-01-27 2011-06-01 台州市尔康药业有限公司 Method for preparing 2-chloropyrimidine

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1385419A (en) * 2002-06-14 2002-12-18 方建文 Process for preparing guanidine hydrochloride
CN102079725A (en) * 2011-01-27 2011-06-01 台州市尔康药业有限公司 Method for preparing 2-chloropyrimidine

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113754567A (en) * 2021-10-13 2021-12-07 宁夏蓝白黑循环科技有限公司 Novel preparation process of refined guanidine carbonate
CN113754567B (en) * 2021-10-13 2024-02-20 宁夏蓝白黑循环科技有限公司 Preparation process of novel refined guanidine carbonate
CN115286538A (en) * 2022-07-12 2022-11-04 烟台三鼎化工有限公司 Antibacterial guanidine hydrochloride efficient crystallization drying process

Similar Documents

Publication Publication Date Title
CN109019691B (en) Preparation process of ammonium paratungstate
CN108101850B (en) Method for improving quality of 5-acetoacetylaminobenzimidazolone
CN101891683B (en) Aminopyrine production method
JP2008543954A (en) Method for producing pentaerythritol
CN106045879B (en) Method for preparing cyanoacetic acid
CN112707848A (en) Preparation method of guanidine hydrochloride
EP3560909B1 (en) Production method for high-quality adipic acid
CN104710375A (en) Method for producing THEIC
CN107365273B (en) Production method for synthesizing 5-nitrobenzimidazole ketone by one-pot method
CN111018747A (en) Method for refining guanidine nitrate
CN103664812A (en) Preparation method of TTZ (thiotriazinone)
CN103172122A (en) Method for purifying high purity ammonium rhenate from liquid containing ammonium rhenate
CN102432456A (en) Synthetic method of fumaric acid
CN113651699B (en) Method for preparing high-purity 2, 4-dinitrochlorobenzene by layered melt crystallization
CN104447758A (en) Synthesis process of pyrazolo[3,4-d]pyrimidine compounds
CN103570522A (en) Method for producing 99.5% of sodium formate
CN110272451B (en) Preparation method of tetraphenylphenol phosphonium salt
CN107963986B (en) Method for co-producing high-purity schofield salt and G salt
CN111233835A (en) Preparation and purification method of 5- (2-fluorophenyl) -1- (pyridine-3-ylsulfonyl) -1H-pyrrole-3-formaldehyde
CN111646904A (en) Method for synthesizing p-nitroanisole
CN114437099A (en) Preparation method of high-purity isosorbide
CN110818546A (en) Method for purifying hydroxypivalaldehyde
CN107778160B (en) Preparation method of 3,4,5, 6-tetrafluorophthalic acid
CN111848433B (en) Process for preparing 4-aminophenylacetamide
CN113683495B (en) Method for preparing 4,4' -dihydroxybenzophenone

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20210427

RJ01 Rejection of invention patent application after publication